# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_MI8
_database_code_depnum_ccdc_archive 'CCDC 2343092'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Nanociencia y Materiales de Aragon (INMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2024-03-25 deposited with the CCDC.	2024-06-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C66 H48 N18 Ni2, 2(B F4), 3(C H4 O), 2(Cl), 4(H2 O)'
_chemical_formula_sum            'C69 H68 B2 Cl2 F8 N18 Ni2 O7'
_chemical_formula_weight         1623.35

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
B B 0.0017 0.0007
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0066 0.0035
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0115 0.0065
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
F F 0.0186 0.0109
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Cl Cl 0.1555 0.1675
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Ni Ni 0.3392 1.1692
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_H-M_alt        'I -4'
_space_group_name_Hall           'I -4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'

_cell_length_a                   29.264(4)
_cell_length_b                   29.264(4)
_cell_length_c                   17.389(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     14892(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9860
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      24.12

_exptl_crystal_description       block
_exptl_crystal_colour            blue-violet
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_F_000             6663
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.685
_shelx_estimated_absorpt_T_min   0.908
_shelx_estimated_absorpt_T_max   0.968
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.642
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_process_details   'SADABS-2016/2 - Bruker AXS'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.72932
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'ALBA XALOC beamline'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'MD2M - Maatel + Dectris PILATUS 6M'
_diffrn_measurement_method       'ω rotation at various κ'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            72518
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_av_R_equivalents  0.0519
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.398
_diffrn_reflns_theta_max         23.887
_diffrn_reflns_theta_full        23.887
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             10667
_reflns_number_gt                8979
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.925
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    0.999

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Global Phasing autoPROC package'
_computing_cell_refinement       'Bruker SAINT v8.38a'
_computing_data_reduction        'Bruker SAINT v8.38a'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;All non-hydrogens were refined anisotropically. 
 Hydrogens were placed geometrically on their carrier atom and refined with 
 a riding model, including those on the pyrazole N (AFIX 43), as no clear
 electron density was present to allow proper free refinement. Hydrogens on the
 lattice water molecules could not be found and are omitted in the structural
 Model but included in the formula.
 One of the Cl anion is disordered over two positions with relative occupancies
 refining to 0.39:0.39 (Cl2A:B). One of the BF4 ion is also disordered
 over two orientations with relative occupancies xxx:xxx (B2A:B2B). These
 were refined with 1,2 and 1,3 distance restraints, as well as displacement 
 parameters restraints. Displacement parameters restraints were used to refine 
 the lattice water and methanol molecules. 
 At the end of the refinement there remained void spaces with only
 weak electron density peaks. Analysis with PLATON/SQUEEZE (see below for details)
 gave two voids of 452 cubic angstrom and two voids of 211 cubic angstroms
 per cell, with 90 and 54 electrons respectively. These figures could 
 correspond to respectively 5 and 3 diffuse methanol molecules per void, for a total
 of 16 per cell, 2 per formula unit. As crystals were freshly taken out of
 their solution, this is reasonable, and was therefore reflected in the 
 reported formula, calculated density, mu etc. Refinement with the squeezed data
 resulted in an improvement in R1 of ca. 1%.

# SQUEEZE RESULTS (Version = 180518)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.000  0.000  0.500       211        64 ' '
   2  0.000  0.500  0.837       452        90 ' '
   3  0.118  0.212  0.387        11        -1 ' '
   4  0.212  0.882  0.613        11        -1 ' '
   5  0.288  0.618  0.113        11        -1 ' '
   6  0.382  0.288  0.887        11        -1 ' '
   7  0.500  1.000  0.124       452        90 ' '
   8  0.500  0.500  0.000       211        64 ' '
   9  0.618  0.712  0.887        11        -1 ' '
  10  0.712  0.382  0.113        11        -1 ' '
  11  0.788  0.118  0.613        11        -1 ' '
  12  0.882  0.788  0.387        11        -1 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           ?,SQUEEZE
;

_vrf_FORMU01_MI8                 
;
PROBLEM: There is a discrepancy between the atom counts in the
            _chemical_formula_sum and the formula from the _atom_site* data.
            Atom count from _chemical_formula_sum:C76 H98 B1 Br3 F4 N18 Ni2 O15
            Atom count from the _atom_site data:  C67 H52 B1 Br3 F4 N18 Ni2 O6      
RESPONSE: PLATON/SQUEEZE has been used to analyse and take into account
the diffuse solvent content, for a total of 9 addition methanol molecules 
per formula unit. Also, hydrogens on the lattice water molecule could not be
found and are omitted in the structural model, but included in the formula. 
This has been reflected in the formula, giving rise to this discrepancy 
between the formula from the atom list and that reported.
;

_vrf_PLAT306_MI8                 
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?)      
RESPONSE: Hydrogens on the lattice water molecule could not be found and 
are indeed omitted in the structural model.
;

_vrf_PLAT090_MI8                 
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       5.58 Note        
RESPONSE: Crystals were relatively poorly diffracting, probably a result of
a large portion of the cell contain diffuse lattice solvent. The present
data were cut at 0.90 angstrom resolution, altogether resulting in relatively
poor theta_max and data over parameter ratio. 
;

_vrf_THETM01_MI8                 
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
            Calculated sin(theta_max)/wavelength =    0.5552       
RESPONSE: Crystals were relatively poorly diffracting, probably a result of
a large portion of the cell contain diffuse lattice solvent. The present
data were cut at 0.90 angstrom resolution, altogether resulting in relatively
poor theta_max and data over parameter ratio. 
;

_vrf_PLAT094_MI8                 
;
PROBLEM: Ratio of Maximum / Minimum Residual Density ....       3.24 Report      
RESPONSE: Some electron density remains at or in the vicinity of 
both Ni sites, which could be due to un-ideal absorption corrections.
;

_vrf_PLAT973_MI8                 
;
PROBLEM: Check Calcd Positive Resid. Density on       Ni1       1.10 eA-3      
RESPONSE: Some electron density remains at or in the vicinity of 
both Ni sites, which could be due to un-ideal absorption corrections.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1888P)²+26.6478P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 3864 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.043(5)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         10667
_refine_ls_number_parameters     993
_refine_ls_number_restraints     251
_refine_ls_R_factor_all          0.1027
_refine_ls_R_factor_gt           0.0882
_refine_ls_wR_factor_ref         0.2539
_refine_ls_wR_factor_gt          0.2311
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.067
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.27715(6) 0.51559(5) 0.36089(9) 0.0580(5) Uani 1 1 d . . . . .
Ni2 Ni 0.14456(6) 0.24412(6) 0.58515(10) 0.0666(5) Uani 1 1 d . . . . .
N1 N 0.2433(4) 0.5785(3) 0.3408(7) 0.064(3) Uani 1 1 d . . . . .
N2 N 0.2387(3) 0.5235(3) 0.4593(6) 0.055(2) Uani 1 1 d . . . . .
N3 N 0.2292(4) 0.4987(3) 0.5216(6) 0.057(2) Uani 1 1 d . . . . .
H3B H 0.244198 0.473854 0.534849 0.068 Uiso 1 1 calc R U . . .
N4 N 0.1493(4) 0.3477(3) 0.6412(6) 0.060(3) Uani 1 1 d . . . . .
H4B H 0.134114 0.359928 0.602695 0.072 Uiso 1 1 calc R U . . .
N5 N 0.1581(4) 0.3036(4) 0.6482(7) 0.069(3) Uani 1 1 d . . . . .
N6 N 0.1778(4) 0.2177(4) 0.6846(6) 0.067(3) Uani 1 1 d . . . . .
N7 N 0.3389(4) 0.5449(4) 0.3964(6) 0.065(3) Uani 1 1 d . . . . .
N8 N 0.3143(3) 0.4596(4) 0.4011(6) 0.060(3) Uani 1 1 d . . . . .
N9 N 0.3101(4) 0.4139(4) 0.4049(6) 0.067(3) Uani 1 1 d . . . . .
H9A H 0.283899 0.399224 0.403187 0.080 Uiso 1 1 calc R U . . .
N10 N 0.2438(4) 0.2708(4) 0.5227(6) 0.068(3) Uani 1 1 d . . . . .
H10B H 0.244309 0.299647 0.537066 0.082 Uiso 1 1 calc R U . . .
N11 N 0.2082(4) 0.2427(4) 0.5304(7) 0.070(3) Uani 1 1 d . . . . .
N12 N 0.1451(5) 0.1786(4) 0.5307(7) 0.070(3) Uani 1 1 d . . . . .
N13 N 0.3040(4) 0.5106(3) 0.2445(6) 0.059(3) Uani 1 1 d . . . . .
N14 N 0.2288(3) 0.4758(3) 0.3054(6) 0.053(2) Uani 1 1 d . . . . .
N15 N 0.1893(3) 0.4555(3) 0.3211(6) 0.053(2) Uani 1 1 d . . . . .
H15A H 0.176327 0.456617 0.366796 0.064 Uiso 1 1 calc R U . . .
N16 N 0.1202(3) 0.3044(3) 0.4405(6) 0.057(2) Uani 1 1 d . . . . .
H16B H 0.148230 0.309919 0.424689 0.068 Uiso 1 1 calc R U . . .
N17 N 0.1094(4) 0.2795(4) 0.5015(6) 0.061(3) Uani 1 1 d . . . . .
N18 N 0.0773(4) 0.2379(4) 0.6227(6) 0.067(3) Uani 1 1 d . . . . .
C1 C 0.2514(6) 0.6071(4) 0.2825(8) 0.072(4) Uani 1 1 d . . . . .
H1A H 0.273210 0.598728 0.244683 0.087 Uiso 1 1 calc R U . . .
C2 C 0.2291(5) 0.6482(5) 0.2754(10) 0.072(4) Uani 1 1 d . . . . .
H2A H 0.235345 0.668051 0.233472 0.087 Uiso 1 1 calc R U . . .
C3 C 0.1971(6) 0.6600(5) 0.3310(10) 0.081(4) Uani 1 1 d . . . . .
H3A H 0.181019 0.688159 0.327248 0.098 Uiso 1 1 calc R U . . .
C4 C 0.1887(5) 0.6306(4) 0.3922(8) 0.065(3) Uani 1 1 d . . . . .
H4A H 0.167041 0.638039 0.430905 0.078 Uiso 1 1 calc R U . . .
C5 C 0.2130(5) 0.5900(4) 0.3948(8) 0.061(3) Uani 1 1 d . . . . .
C6 C 0.2087(4) 0.5569(4) 0.4602(7) 0.055(3) Uani 1 1 d . . . . .
C7 C 0.1807(4) 0.5546(4) 0.5212(7) 0.055(3) Uani 1 1 d . . . . .
H7A H 0.156637 0.575118 0.533486 0.066 Uiso 1 1 calc R U . . .
C8 C 0.1936(4) 0.5165(4) 0.5623(7) 0.055(3) Uani 1 1 d . . . . .
C9 C 0.1779(4) 0.4930(5) 0.6333(8) 0.062(3) Uani 1 1 d . . . . .
C10 C 0.1643(5) 0.5165(5) 0.6966(9) 0.074(4) Uani 1 1 d . . . . .
H10A H 0.163490 0.548955 0.695176 0.089 Uiso 1 1 calc R U . . .
C11 C 0.1517(6) 0.4940(7) 0.7629(11) 0.091(5) Uani 1 1 d . . . . .
H11A H 0.142533 0.511402 0.806421 0.109 Uiso 1 1 calc R U . . .
C12 C 0.1520(6) 0.4456(6) 0.7681(9) 0.079(4) Uani 1 1 d . . . . .
H12A H 0.143554 0.430238 0.814030 0.095 Uiso 1 1 calc R U . . .
C13 C 0.1655(5) 0.4213(5) 0.7013(8) 0.070(4) Uani 1 1 d . . . . .
C14 C 0.1769(4) 0.4455(4) 0.6336(8) 0.057(3) Uani 1 1 d . . . . .
H14A H 0.184041 0.429159 0.587971 0.069 Uiso 1 1 calc R U . . .
C15 C 0.1664(4) 0.3708(4) 0.6995(8) 0.060(3) Uani 1 1 d . . . . .
C16 C 0.1872(5) 0.3397(6) 0.7462(8) 0.073(4) Uani 1 1 d . . . . .
H16A H 0.202904 0.345512 0.793029 0.087 Uiso 1 1 calc R U . . .
C17 C 0.1804(4) 0.2974(5) 0.7106(7) 0.061(3) Uani 1 1 d . . . . .
C18 C 0.1954(5) 0.2504(5) 0.7297(9) 0.070(4) Uani 1 1 d . . . . .
C19 C 0.2262(5) 0.2407(5) 0.7866(8) 0.067(3) Uani 1 1 d . . . . .
H19A H 0.239165 0.264319 0.816980 0.081 Uiso 1 1 calc R U . . .
C20 C 0.2380(5) 0.1946(6) 0.7987(9) 0.075(4) Uani 1 1 d . . . . .
H20A H 0.259257 0.186825 0.837838 0.090 Uiso 1 1 calc R U . . .
C21 C 0.2192(6) 0.1611(6) 0.7546(9) 0.079(4) Uani 1 1 d . . . . .
H21A H 0.226345 0.129927 0.763778 0.095 Uiso 1 1 calc R U . . .
C22 C 0.1898(5) 0.1730(5) 0.6966(8) 0.071(4) Uani 1 1 d . . . . .
H22A H 0.177437 0.149943 0.664321 0.085 Uiso 1 1 calc R U . . .
C23 C 0.3482(6) 0.5900(6) 0.3992(8) 0.081(4) Uani 1 1 d . . . . .
H23A H 0.324031 0.611360 0.393208 0.097 Uiso 1 1 calc R U . . .
C24 C 0.3929(6) 0.6059(7) 0.4108(10) 0.093(5) Uani 1 1 d . . . . .
H24A H 0.398468 0.637780 0.415821 0.112 Uiso 1 1 calc R U . . .
C25 C 0.4295(6) 0.5749(7) 0.4149(11) 0.091(5) Uani 1 1 d . . . . .
H25A H 0.460234 0.585089 0.418155 0.110 Uiso 1 1 calc R U . . .
C26 C 0.4190(6) 0.5300(7) 0.4139(10) 0.090(5) Uani 1 1 d . . . . .
H26A H 0.442585 0.508031 0.419762 0.108 Uiso 1 1 calc R U . . .
C27 C 0.3728(5) 0.5152(6) 0.4042(8) 0.071(4) Uani 1 1 d . . . . .
C28 C 0.3594(5) 0.4681(5) 0.4041(8) 0.067(3) Uani 1 1 d . . . . .
C29 C 0.3841(5) 0.4275(6) 0.4113(8) 0.072(4) Uani 1 1 d . . . . .
H29A H 0.416327 0.423993 0.415276 0.087 Uiso 1 1 calc R U . . .
C30 C 0.3511(4) 0.3935(5) 0.4115(8) 0.068(4) Uani 1 1 d . . . . .
C31 C 0.3548(5) 0.3441(5) 0.4210(8) 0.072(4) Uani 1 1 d . . . . .
C32 C 0.3906(5) 0.3190(5) 0.3903(8) 0.072(4) Uani 1 1 d . . . . .
H32A H 0.414694 0.334837 0.365148 0.087 Uiso 1 1 calc R U . . .
C33 C 0.3928(6) 0.2734(7) 0.3946(11) 0.091(5) Uani 1 1 d . . . . .
H33A H 0.418671 0.258010 0.374256 0.110 Uiso 1 1 calc R U . . .
C34 C 0.3574(5) 0.2479(6) 0.4288(9) 0.080(4) Uani 1 1 d . . . . .
H34A H 0.358269 0.215427 0.430192 0.096 Uiso 1 1 calc R U . . .
C35 C 0.3198(5) 0.2730(6) 0.4615(8) 0.077(4) Uani 1 1 d . . . . .
C36 C 0.3206(5) 0.3190(5) 0.4575(8) 0.066(3) Uani 1 1 d . . . . .
H36A H 0.296339 0.335325 0.481150 0.079 Uiso 1 1 calc R U . . .
C37 C 0.2796(5) 0.2476(5) 0.4889(8) 0.066(3) Uani 1 1 d . . . . .
C38 C 0.2658(5) 0.2053(6) 0.4750(10) 0.082(4) Uani 1 1 d . . . . .
H38A H 0.282950 0.181373 0.451752 0.098 Uiso 1 1 calc R U . . .
C39 C 0.2203(5) 0.2031(4) 0.5021(8) 0.068(4) Uani 1 1 d . . . . .
C40 C 0.1845(6) 0.1666(5) 0.5004(8) 0.076(4) Uani 1 1 d . . . . .
C41 C 0.1925(7) 0.1244(5) 0.4665(10) 0.085(4) Uani 1 1 d . . . . .
H41A H 0.221561 0.116595 0.445932 0.102 Uiso 1 1 calc R U . . .
C42 C 0.1564(6) 0.0946(6) 0.4642(9) 0.082(4) Uani 1 1 d . . . . .
H42A H 0.159861 0.065771 0.439793 0.098 Uiso 1 1 calc R U . . .
C43 C 0.1154(6) 0.1062(5) 0.4967(10) 0.081(4) Uani 1 1 d . . . . .
H43A H 0.090687 0.085124 0.496973 0.098 Uiso 1 1 calc R U . . .
C44 C 0.1107(6) 0.1488(6) 0.5289(9) 0.080(4) Uani 1 1 d . . . . .
H44A H 0.082156 0.157209 0.550546 0.097 Uiso 1 1 calc R U . . .
C45 C 0.3417(6) 0.5309(5) 0.2175(8) 0.073(4) Uani 1 1 d . . . . .
H45A H 0.359789 0.548805 0.251396 0.087 Uiso 1 1 calc R U . . .
C46 C 0.3550(6) 0.5265(5) 0.1409(11) 0.083(4) Uani 1 1 d . . . . .
H46A H 0.381727 0.541342 0.122510 0.100 Uiso 1 1 calc R U . . .
C47 C 0.3291(5) 0.5005(6) 0.0933(8) 0.079(4) Uani 1 1 d . . . . .
H47A H 0.338178 0.496726 0.041177 0.094 Uiso 1 1 calc R U . . .
C48 C 0.2900(5) 0.4795(5) 0.1191(9) 0.071(4) Uani 1 1 d . . . . .
H48A H 0.271234 0.461838 0.086057 0.086 Uiso 1 1 calc R U . . .
C49 C 0.2795(5) 0.4857(4) 0.1970(7) 0.058(3) Uani 1 1 d . . . . .
C50 C 0.2373(4) 0.4664(4) 0.2308(7) 0.053(3) Uani 1 1 d . . . . .
C51 C 0.2018(4) 0.4397(4) 0.1996(7) 0.054(3) Uani 1 1 d . . . . .
H51A H 0.199345 0.428646 0.148420 0.064 Uiso 1 1 calc R U . . .
C52 C 0.1706(4) 0.4330(4) 0.2607(7) 0.052(3) Uani 1 1 d . . . . .
C53 C 0.1291(5) 0.4067(4) 0.2665(7) 0.056(3) Uani 1 1 d . . . . .
C54 C 0.0942(5) 0.4097(5) 0.2116(7) 0.065(3) Uani 1 1 d . . . . .
H54A H 0.096875 0.429950 0.169093 0.077 Uiso 1 1 calc R U . . .
C55 C 0.0557(5) 0.3827(5) 0.2206(8) 0.072(4) Uani 1 1 d . . . . .
H55A H 0.032397 0.383474 0.182582 0.087 Uiso 1 1 calc R U . . .
C56 C 0.0507(4) 0.3549(5) 0.2836(8) 0.067(3) Uani 1 1 d . . . . .
H56A H 0.023709 0.337168 0.289069 0.081 Uiso 1 1 calc R U . . .
C57 C 0.0845(4) 0.3524(4) 0.3395(6) 0.053(3) Uani 1 1 d . . . . .
C58 C 0.1238(4) 0.3786(4) 0.3309(7) 0.053(3) Uani 1 1 d . . . . .
H58A H 0.147103 0.377401 0.368878 0.064 Uiso 1 1 calc R U . . .
C59 C 0.0807(4) 0.3207(4) 0.4048(7) 0.057(3) Uani 1 1 d . . . . .
C60 C 0.0452(5) 0.3032(4) 0.4463(8) 0.060(3) Uani 1 1 d . . . . .
H60A H 0.013559 0.306875 0.436114 0.072 Uiso 1 1 calc R U . . .
C61 C 0.0649(4) 0.2787(4) 0.5069(7) 0.058(3) Uani 1 1 d . . . . .
C62 C 0.0445(5) 0.2548(5) 0.5734(8) 0.071(4) Uani 1 1 d . . . . .
C63 C -0.0012(5) 0.2528(5) 0.5900(10) 0.076(4) Uani 1 1 d . . . . .
H63A H -0.023257 0.264562 0.555117 0.091 Uiso 1 1 calc R U . . .
C64 C -0.0143(6) 0.2332(5) 0.6581(10) 0.076(4) Uani 1 1 d . . . . .
H64A H -0.045880 0.231790 0.670327 0.091 Uiso 1 1 calc R U . . .
C65 C 0.0149(6) 0.2167(7) 0.7064(11) 0.091(5) Uani 1 1 d . . . . .
H65A H 0.005264 0.203545 0.753595 0.109 Uiso 1 1 calc R U . . .
C66 C 0.0620(6) 0.2188(6) 0.6865(9) 0.084(4) Uani 1 1 d . . . . .
H66A H 0.083635 0.205801 0.720894 0.101 Uiso 1 1 calc R U . . .
Cl1 Cl 0.21300(11) 0.37029(11) 0.46487(18) 0.0634(8) Uani 1 1 d . . . . .
Cl2A Cl 0.1194(4) 0.4704(3) 0.4426(5) 0.103(4) Uani 0.491(16) 1 d . U P A 1
Cl2B Cl 0.0842(6) 0.3981(4) 0.5451(7) 0.155(7) Uani 0.509(16) 1 d . U P A 2
B1 B 0.3141(8) 0.3512(8) 0.7447(12) 0.093(6) Uani 1 1 d . . . . .
F1 F 0.2923(6) 0.3968(5) 0.7378(8) 0.140(5) Uani 1 1 d . . . . .
F2 F 0.2907(5) 0.3293(6) 0.8041(8) 0.142(5) Uani 1 1 d . . . . .
F3 F 0.3074(6) 0.3307(5) 0.6782(8) 0.135(4) Uani 1 1 d . . . . .
F4 F 0.3586(4) 0.3590(5) 0.7629(8) 0.121(4) Uani 1 1 d . . . . .
B2A B 0.1584(8) 0.4159(6) -0.0175(13) 0.094(3) Uani 0.838(11) 1 d D U P B 1
F5A F 0.1529(4) 0.3786(4) -0.0634(7) 0.098(3) Uani 0.838(11) 1 d D U P B 1
F6A F 0.1988(4) 0.4167(5) 0.0165(7) 0.110(3) Uani 0.838(11) 1 d D U P B 1
F7A F 0.1495(4) 0.4561(4) -0.0565(7) 0.101(3) Uani 0.838(11) 1 d D U P B 1
F8A F 0.1222(5) 0.4138(5) 0.0376(8) 0.119(4) Uani 0.838(11) 1 d D U P B 1
B2B B 0.1292(15) 0.4110(14) -0.023(2) 0.107(6) Uani 0.162(11) 1 d D U P B 2
F5B F 0.118(2) 0.407(2) -0.099(2) 0.113(8) Uani 0.162(11) 1 d D U P B 2
F6B F 0.1748(15) 0.4037(18) -0.015(3) 0.092(7) Uani 0.162(11) 1 d D U P B 2
F7B F 0.1180(19) 0.4536(15) 0.001(3) 0.109(8) Uani 0.162(11) 1 d D U P B 2
F8B F 0.1057(19) 0.3793(18) 0.019(3) 0.115(8) Uani 0.162(11) 1 d D U P B 2
O1W O 0.2947(6) 0.4449(7) 0.5957(9) 0.152(7) Uani 1 1 d . U . . .
O2W O 0.3977(7) 0.4448(6) 0.7847(11) 0.141(6) Uani 1 1 d . . . . .
O3W O 0.3757(4) 0.5130(3) 0.6570(7) 0.087(3) Uani 1 1 d . . . . .
O4W O 0.3981(6) 0.5064(4) 0.9160(9) 0.119(5) Uani 1 1 d . U . . .
O1S O 0.3892(8) 0.5765(6) 0.7897(12) 0.154(7) Uani 1 1 d . . . . .
H1S H 0.398025 0.549178 0.791094 0.231 Uiso 1 1 d R U . . .
C1S C 0.4228(10) 0.6034(12) 0.7955(18) 0.152(11) Uani 1 1 d . . . . .
H1S1 H 0.413922 0.634384 0.780140 0.229 Uiso 1 1 d R U . . .
H1S2 H 0.447082 0.592354 0.761460 0.229 Uiso 1 1 d R U . . .
H1S3 H 0.433902 0.603824 0.848660 0.229 Uiso 1 1 d R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N2 2.061(10) . ?
Ni1 N14 2.071(10) . ?
Ni1 N8 2.087(11) . ?
Ni1 N7 2.094(11) . ?
Ni1 N1 2.119(10) . ?
Ni1 N13 2.176(10) . ?
Ni2 N17 2.060(10) . ?
Ni2 N18 2.083(12) . ?
Ni2 N11 2.093(13) . ?
Ni2 N5 2.095(13) . ?
Ni2 N6 2.130(10) . ?
Ni2 N12 2.139(11) . ?
N1 C1 1.335(17) . ?
N1 C5 1.335(18) . ?
N2 C6 1.313(16) . ?
N2 N3 1.332(15) . ?
N3 C8 1.365(16) . ?
N3 H3B 0.8800 . ?
N4 C15 1.319(18) . ?
N4 N5 1.321(15) . ?
N4 H4B 0.8800 . ?
N5 C17 1.279(18) . ?
N6 C18 1.34(2) . ?
N6 C22 1.370(19) . ?
N7 C27 1.326(19) . ?
N7 C23 1.35(2) . ?
N8 N9 1.343(16) . ?
N8 C28 1.345(18) . ?
N9 C30 1.345(17) . ?
N9 H9A 0.8800 . ?
N10 N11 1.332(17) . ?
N10 C37 1.382(18) . ?
N10 H10B 0.8800 . ?
N11 C39 1.309(18) . ?
N12 C40 1.32(2) . ?
N12 C44 1.33(2) . ?
N13 C49 1.315(17) . ?
N13 C45 1.337(19) . ?
N14 N15 1.329(14) . ?
N14 C50 1.349(15) . ?
N15 C52 1.355(16) . ?
N15 H15A 0.8800 . ?
N16 N17 1.326(15) . ?
N16 C59 1.396(16) . ?
N16 H16B 0.8800 . ?
N17 C61 1.307(17) . ?
N18 C66 1.319(19) . ?
N18 C62 1.378(18) . ?
C1 C2 1.37(2) . ?
C1 H1A 0.9500 . ?
C2 C3 1.39(2) . ?
C2 H2A 0.9500 . ?
C3 C4 1.39(2) . ?
C3 H3A 0.9500 . ?
C4 C5 1.384(19) . ?
C4 H4A 0.9500 . ?
C5 C6 1.500(18) . ?
C6 C7 1.343(18) . ?
C7 C8 1.376(18) . ?
C7 H7A 0.9500 . ?
C8 C9 1.485(19) . ?
C9 C10 1.36(2) . ?
C9 C14 1.391(19) . ?
C10 C11 1.38(2) . ?
C10 H10A 0.9500 . ?
C11 C12 1.42(3) . ?
C11 H11A 0.9500 . ?
C12 C13 1.42(2) . ?
C12 H12A 0.9500 . ?
C13 C14 1.41(2) . ?
C13 C15 1.48(2) . ?
C14 H14A 0.9500 . ?
C15 C16 1.36(2) . ?
C16 C17 1.40(2) . ?
C16 H16A 0.9500 . ?
C17 C18 1.48(2) . ?
C18 C19 1.37(2) . ?
C19 C20 1.41(2) . ?
C19 H19A 0.9500 . ?
C20 C21 1.36(2) . ?
C20 H20A 0.9500 . ?
C21 C22 1.37(2) . ?
C21 H21A 0.9500 . ?
C22 H22A 0.9500 . ?
C23 C24 1.40(2) . ?
C23 H23A 0.9500 . ?
C24 C25 1.41(3) . ?
C24 H24A 0.9500 . ?
C25 C26 1.35(3) . ?
C25 H25A 0.9500 . ?
C26 C27 1.43(2) . ?
C26 H26A 0.9500 . ?
C27 C28 1.43(2) . ?
C28 C29 1.40(2) . ?
C29 C30 1.39(2) . ?
C29 H29A 0.9500 . ?
C30 C31 1.46(2) . ?
C31 C32 1.39(2) . ?
C31 C36 1.39(2) . ?
C32 C33 1.34(2) . ?
C32 H32A 0.9500 . ?
C33 C34 1.41(2) . ?
C33 H33A 0.9500 . ?
C34 C35 1.44(2) . ?
C34 H34A 0.9500 . ?
C35 C36 1.35(2) . ?
C35 C37 1.47(2) . ?
C36 H36A 0.9500 . ?
C37 C38 1.33(2) . ?
C38 C39 1.42(2) . ?
C38 H38A 0.9500 . ?
C39 C40 1.50(2) . ?
C40 C41 1.39(2) . ?
C41 C42 1.37(3) . ?
C41 H41A 0.9500 . ?
C42 C43 1.37(3) . ?
C42 H42A 0.9500 . ?
C43 C44 1.37(2) . ?
C43 H43A 0.9500 . ?
C44 H44A 0.9500 . ?
C45 C46 1.39(2) . ?
C45 H45A 0.9500 . ?
C46 C47 1.36(2) . ?
C46 H46A 0.9500 . ?
C47 C48 1.37(2) . ?
C47 H47A 0.9500 . ?
C48 C49 1.40(2) . ?
C48 H48A 0.9500 . ?
C49 C50 1.479(18) . ?
C50 C51 1.408(18) . ?
C51 C52 1.414(17) . ?
C51 H51A 0.9500 . ?
C52 C53 1.444(18) . ?
C53 C58 1.398(17) . ?
C53 C54 1.400(19) . ?
C54 C55 1.38(2) . ?
C54 H54A 0.9500 . ?
C55 C56 1.37(2) . ?
C55 H55A 0.9500 . ?
C56 C57 1.389(18) . ?
C56 H56A 0.9500 . ?
C57 C58 1.390(18) . ?
C57 C59 1.469(17) . ?
C58 H58A 0.9500 . ?
C59 C60 1.364(18) . ?
C60 C61 1.399(18) . ?
C60 H60A 0.9500 . ?
C61 C62 1.476(19) . ?
C62 C63 1.37(2) . ?
C63 C64 1.37(2) . ?
C63 H63A 0.9500 . ?
C64 C65 1.29(2) . ?
C64 H64A 0.9500 . ?
C65 C66 1.42(3) . ?
C65 H65A 0.9500 . ?
C66 H66A 0.9500 . ?
B1 F3 1.32(3) . ?
B1 F4 1.36(3) . ?
B1 F2 1.39(3) . ?
B1 F1 1.49(3) . ?
B2A F6A 1.322(19) . ?
B2A F5A 1.362(19) . ?
B2A F7A 1.382(18) . ?
B2A F8A 1.43(3) . ?
B2B F7B 1.36(3) . ?
B2B F6B 1.36(3) . ?
B2B F8B 1.36(3) . ?
B2B F5B 1.36(3) . ?
O1S C1S 1.26(3) . ?
O1S H1S 0.8402 . ?
C1S H1S1 0.9801 . ?
C1S H1S2 0.9798 . ?
C1S H1S3 0.9802 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Ni1 N14 94.4(4) . . ?
N2 Ni1 N8 95.4(4) . . ?
N14 Ni1 N8 94.0(4) . . ?
N2 Ni1 N7 100.5(4) . . ?
N14 Ni1 N7 163.2(4) . . ?
N8 Ni1 N7 76.9(5) . . ?
N2 Ni1 N1 77.5(4) . . ?
N14 Ni1 N1 95.3(4) . . ?
N8 Ni1 N1 168.7(4) . . ?
N7 Ni1 N1 95.5(5) . . ?
N2 Ni1 N13 167.7(4) . . ?
N14 Ni1 N13 77.1(4) . . ?
N8 Ni1 N13 94.1(4) . . ?
N7 Ni1 N13 89.4(4) . . ?
N1 Ni1 N13 94.2(4) . . ?
N17 Ni2 N18 78.1(4) . . ?
N17 Ni2 N11 97.6(4) . . ?
N18 Ni2 N11 169.3(5) . . ?
N17 Ni2 N5 92.7(4) . . ?
N18 Ni2 N5 95.0(5) . . ?
N11 Ni2 N5 94.9(5) . . ?
N17 Ni2 N6 169.6(5) . . ?
N18 Ni2 N6 98.4(4) . . ?
N11 Ni2 N6 87.5(4) . . ?
N5 Ni2 N6 77.8(5) . . ?
N17 Ni2 N12 98.1(4) . . ?
N18 Ni2 N12 93.8(5) . . ?
N11 Ni2 N12 77.0(5) . . ?
N5 Ni2 N12 167.3(5) . . ?
N6 Ni2 N12 91.8(5) . . ?
C1 N1 C5 119.5(11) . . ?
C1 N1 Ni1 126.0(10) . . ?
C5 N1 Ni1 114.5(8) . . ?
C6 N2 N3 104.9(10) . . ?
C6 N2 Ni1 117.3(8) . . ?
N3 N2 Ni1 136.6(7) . . ?
N2 N3 C8 111.9(9) . . ?
N2 N3 H3B 124.1 . . ?
C8 N3 H3B 124.1 . . ?
C15 N4 N5 110.9(10) . . ?
C15 N4 H4B 124.6 . . ?
N5 N4 H4B 124.6 . . ?
C17 N5 N4 108.5(12) . . ?
C17 N5 Ni2 115.0(9) . . ?
N4 N5 Ni2 136.5(9) . . ?
C18 N6 C22 119.7(12) . . ?
C18 N6 Ni2 113.1(9) . . ?
C22 N6 Ni2 125.9(11) . . ?
C27 N7 C23 119.2(13) . . ?
C27 N7 Ni1 114.1(10) . . ?
C23 N7 Ni1 125.8(11) . . ?
N9 N8 C28 105.7(11) . . ?
N9 N8 Ni1 138.7(9) . . ?
C28 N8 Ni1 112.2(9) . . ?
N8 N9 C30 111.5(12) . . ?
N8 N9 H9A 124.2 . . ?
C30 N9 H9A 124.2 . . ?
N11 N10 C37 109.5(12) . . ?
N11 N10 H10B 125.3 . . ?
C37 N10 H10B 125.3 . . ?
C39 N11 N10 107.4(12) . . ?
C39 N11 Ni2 115.3(10) . . ?
N10 N11 Ni2 136.8(9) . . ?
C40 N12 C44 118.5(14) . . ?
C40 N12 Ni2 115.0(10) . . ?
C44 N12 Ni2 126.4(12) . . ?
C49 N13 C45 118.4(11) . . ?
C49 N13 Ni1 115.1(8) . . ?
C45 N13 Ni1 126.5(9) . . ?
N15 N14 C50 105.5(9) . . ?
N15 N14 Ni1 138.6(8) . . ?
C50 N14 Ni1 115.9(8) . . ?
N14 N15 C52 114.1(10) . . ?
N14 N15 H15A 123.0 . . ?
C52 N15 H15A 123.0 . . ?
N17 N16 C59 110.3(10) . . ?
N17 N16 H16B 124.8 . . ?
C59 N16 H16B 124.8 . . ?
C61 N17 N16 107.7(9) . . ?
C61 N17 Ni2 116.0(8) . . ?
N16 N17 Ni2 136.3(8) . . ?
C66 N18 C62 116.1(13) . . ?
C66 N18 Ni2 128.3(10) . . ?
C62 N18 Ni2 115.5(9) . . ?
N1 C1 C2 122.3(15) . . ?
N1 C1 H1A 118.9 . . ?
C2 C1 H1A 118.9 . . ?
C1 C2 C3 118.4(14) . . ?
C1 C2 H2A 120.8 . . ?
C3 C2 H2A 120.8 . . ?
C2 C3 C4 119.8(14) . . ?
C2 C3 H3A 120.1 . . ?
C4 C3 H3A 120.1 . . ?
C5 C4 C3 117.7(14) . . ?
C5 C4 H4A 121.1 . . ?
C3 C4 H4A 121.1 . . ?
N1 C5 C4 122.4(12) . . ?
N1 C5 C6 115.2(11) . . ?
C4 C5 C6 122.4(13) . . ?
N2 C6 C7 112.3(11) . . ?
N2 C6 C5 114.6(11) . . ?
C7 C6 C5 133.1(12) . . ?
C6 C7 C8 106.5(11) . . ?
C6 C7 H7A 126.7 . . ?
C8 C7 H7A 126.7 . . ?
N3 C8 C7 104.4(10) . . ?
N3 C8 C9 119.4(10) . . ?
C7 C8 C9 136.2(12) . . ?
C10 C9 C14 119.8(14) . . ?
C10 C9 C8 122.0(12) . . ?
C14 C9 C8 118.2(11) . . ?
C9 C10 C11 121.0(15) . . ?
C9 C10 H10A 119.5 . . ?
C11 C10 H10A 119.5 . . ?
C10 C11 C12 121.8(15) . . ?
C10 C11 H11A 119.1 . . ?
C12 C11 H11A 119.1 . . ?
C13 C12 C11 116.8(15) . . ?
C13 C12 H12A 121.6 . . ?
C11 C12 H12A 121.6 . . ?
C14 C13 C12 119.8(14) . . ?
C14 C13 C15 118.6(12) . . ?
C12 C13 C15 121.6(13) . . ?
C9 C14 C13 120.6(13) . . ?
C9 C14 H14A 119.7 . . ?
C13 C14 H14A 119.7 . . ?
N4 C15 C16 106.6(12) . . ?
N4 C15 C13 121.5(11) . . ?
C16 C15 C13 131.6(14) . . ?
C15 C16 C17 105.3(13) . . ?
C15 C16 H16A 127.4 . . ?
C17 C16 H16A 127.4 . . ?
N5 C17 C16 108.8(12) . . ?
N5 C17 C18 118.3(13) . . ?
C16 C17 C18 132.9(13) . . ?
N6 C18 C19 121.9(13) . . ?
N6 C18 C17 114.7(12) . . ?
C19 C18 C17 123.3(16) . . ?
C18 C19 C20 117.9(15) . . ?
C18 C19 H19A 121.0 . . ?
C20 C19 H19A 121.0 . . ?
C21 C20 C19 120.4(14) . . ?
C21 C20 H20A 119.8 . . ?
C19 C20 H20A 119.8 . . ?
C20 C21 C22 119.0(15) . . ?
C20 C21 H21A 120.5 . . ?
C22 C21 H21A 120.5 . . ?
C21 C22 N6 121.0(16) . . ?
C21 C22 H22A 119.5 . . ?
N6 C22 H22A 119.5 . . ?
N7 C23 C24 121.2(18) . . ?
N7 C23 H23A 119.4 . . ?
C24 C23 H23A 119.4 . . ?
C23 C24 C25 120.1(17) . . ?
C23 C24 H24A 119.9 . . ?
C25 C24 H24A 119.9 . . ?
C26 C25 C24 117.1(16) . . ?
C26 C25 H25A 121.5 . . ?
C24 C25 H25A 121.5 . . ?
C25 C26 C27 120.9(17) . . ?
C25 C26 H26A 119.6 . . ?
C27 C26 H26A 119.6 . . ?
N7 C27 C26 121.3(16) . . ?
N7 C27 C28 115.1(12) . . ?
C26 C27 C28 123.6(15) . . ?
N8 C28 C29 110.8(13) . . ?
N8 C28 C27 116.6(12) . . ?
C29 C28 C27 132.4(14) . . ?
C30 C29 C28 104.4(12) . . ?
C30 C29 H29A 127.8 . . ?
C28 C29 H29A 127.8 . . ?
N9 C30 C29 107.5(13) . . ?
N9 C30 C31 121.1(14) . . ?
C29 C30 C31 131.3(12) . . ?
C32 C31 C36 115.9(14) . . ?
C32 C31 C30 122.5(14) . . ?
C36 C31 C30 121.4(12) . . ?
C33 C32 C31 122.9(16) . . ?
C33 C32 H32A 118.6 . . ?
C31 C32 H32A 118.6 . . ?
C32 C33 C34 121.2(14) . . ?
C32 C33 H33A 119.4 . . ?
C34 C33 H33A 119.4 . . ?
C33 C34 C35 117.2(15) . . ?
C33 C34 H34A 121.4 . . ?
C35 C34 H34A 121.4 . . ?
C36 C35 C34 118.4(16) . . ?
C36 C35 C37 122.4(11) . . ?
C34 C35 C37 118.7(15) . . ?
C35 C36 C31 124.3(12) . . ?
C35 C36 H36A 117.9 . . ?
C31 C36 H36A 117.9 . . ?
C38 C37 N10 107.7(14) . . ?
C38 C37 C35 131.1(14) . . ?
N10 C37 C35 119.9(13) . . ?
C37 C38 C39 105.6(13) . . ?
C37 C38 H38A 127.2 . . ?
C39 C38 H38A 127.2 . . ?
N11 C39 C38 109.8(13) . . ?
N11 C39 C40 116.9(14) . . ?
C38 C39 C40 133.2(14) . . ?
N12 C40 C41 123.7(16) . . ?
N12 C40 C39 114.6(13) . . ?
C41 C40 C39 121.7(16) . . ?
C42 C41 C40 116.6(17) . . ?
C42 C41 H41A 121.7 . . ?
C40 C41 H41A 121.7 . . ?
C43 C42 C41 120.4(16) . . ?
C43 C42 H42A 119.8 . . ?
C41 C42 H42A 119.8 . . ?
C42 C43 C44 118.7(16) . . ?
C42 C43 H43A 120.7 . . ?
C44 C43 H43A 120.7 . . ?
N12 C44 C43 122.0(16) . . ?
N12 C44 H44A 119.0 . . ?
C43 C44 H44A 119.0 . . ?
N13 C45 C46 121.7(14) . . ?
N13 C45 H45A 119.2 . . ?
C46 C45 H45A 119.2 . . ?
C47 C46 C45 118.7(14) . . ?
C47 C46 H46A 120.7 . . ?
C45 C46 H46A 120.7 . . ?
C46 C47 C48 121.0(14) . . ?
C46 C47 H47A 119.5 . . ?
C48 C47 H47A 119.5 . . ?
C47 C48 C49 116.3(15) . . ?
C47 C48 H48A 121.8 . . ?
C49 C48 H48A 121.8 . . ?
N13 C49 C48 123.9(13) . . ?
N13 C49 C50 114.7(10) . . ?
C48 C49 C50 121.3(13) . . ?
N14 C50 C51 110.3(10) . . ?
N14 C50 C49 117.3(11) . . ?
C51 C50 C49 132.4(11) . . ?
C50 C51 C52 105.3(10) . . ?
C50 C51 H51A 127.4 . . ?
C52 C51 H51A 127.4 . . ?
N15 C52 C51 104.8(10) . . ?
N15 C52 C53 123.0(11) . . ?
C51 C52 C53 132.1(11) . . ?
C58 C53 C54 120.2(12) . . ?
C58 C53 C52 117.6(11) . . ?
C54 C53 C52 122.2(11) . . ?
C55 C54 C53 118.6(11) . . ?
C55 C54 H54A 120.7 . . ?
C53 C54 H54A 120.7 . . ?
C56 C55 C54 121.0(12) . . ?
C56 C55 H55A 119.5 . . ?
C54 C55 H55A 119.5 . . ?
C55 C56 C57 121.0(12) . . ?
C55 C56 H56A 119.5 . . ?
C57 C56 H56A 119.5 . . ?
C56 C57 C58 118.9(11) . . ?
C56 C57 C59 121.4(11) . . ?
C58 C57 C59 119.6(11) . . ?
C57 C58 C53 120.1(11) . . ?
C57 C58 H58A 119.9 . . ?
C53 C58 H58A 119.9 . . ?
C60 C59 N16 105.4(11) . . ?
C60 C59 C57 134.7(12) . . ?
N16 C59 C57 119.7(11) . . ?
C59 C60 C61 106.2(11) . . ?
C59 C60 H60A 126.9 . . ?
C61 C60 H60A 126.9 . . ?
N17 C61 C60 110.3(11) . . ?
N17 C61 C62 117.9(11) . . ?
C60 C61 C62 131.8(12) . . ?
C63 C62 N18 122.2(13) . . ?
C63 C62 C61 125.4(13) . . ?
N18 C62 C61 112.1(12) . . ?
C64 C63 C62 118.2(14) . . ?
C64 C63 H63A 120.9 . . ?
C62 C63 H63A 120.9 . . ?
C65 C64 C63 122.2(16) . . ?
C65 C64 H64A 118.9 . . ?
C63 C64 H64A 118.9 . . ?
C64 C65 C66 117.8(16) . . ?
C64 C65 H65A 121.1 . . ?
C66 C65 H65A 121.1 . . ?
N18 C66 C65 123.4(15) . . ?
N18 C66 H66A 118.3 . . ?
C65 C66 H66A 118.3 . . ?
F3 B1 F4 115(2) . . ?
F3 B1 F2 111.7(19) . . ?
F4 B1 F2 112.0(15) . . ?
F3 B1 F1 105.9(15) . . ?
F4 B1 F1 106.1(18) . . ?
F2 B1 F1 105.1(19) . . ?
F6A B2A F5A 112.3(17) . . ?
F6A B2A F7A 111.9(15) . . ?
F5A B2A F7A 111.8(15) . . ?
F6A B2A F8A 111.3(16) . . ?
F5A B2A F8A 105.7(15) . . ?
F7A B2A F8A 103.2(16) . . ?
F7B B2B F6B 110.4(19) . . ?
F7B B2B F8B 109.7(19) . . ?
F6B B2B F8B 109.7(19) . . ?
F7B B2B F5B 108.8(19) . . ?
F6B B2B F5B 108.9(19) . . ?
F8B B2B F5B 109.3(19) . . ?
C1S O1S H1S 110.7 . . ?
O1S C1S H1S1 110.4 . . ?
O1S C1S H1S2 108.1 . . ?
H1S1 C1S H1S2 109.4 . . ?
O1S C1S H1S3 110.0 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3B O1W 0.88 2.00 2.794(16) 148.7 . yes
N4 H4B Cl2B^b 0.88 2.09 2.932(16) 159.1 . yes
N9 H9A Cl1 0.88 2.48 3.286(12) 151.7 . yes
N10 H10B Cl1 0.88 2.59 3.209(11) 128.5 . yes
N15 H15A Cl2A^a 0.88 2.16 2.971(14) 152.6 . yes
N16 H16B Cl1 0.88 2.68 3.357(11) 134.2 . yes
O1S H1S O4W 0.84 2.51 3.02(2) 120.1 . yes

_refine_diff_density_max         1.535
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.142



####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_MI7
_database_code_depnum_ccdc_archive 'CCDC 2343093'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Nanociencia y Materiales de Aragon (INMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2024-03-25 deposited with the CCDC.	2024-06-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C66 H48 N18 Ni2, B F4, 3(Br), 10(C H4 O), 5(H2 O)'
_chemical_formula_sum            'C76 H98 B Br3 F4 N18 Ni2 O15'
_chemical_formula_weight         1947.66

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
B B 0.0017 0.0007
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0066 0.0035
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0115 0.0065
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
F F 0.0186 0.0109
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Br Br -0.4703 2.5520
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Ni Ni 0.3377 1.1698
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_H-M_alt        'I -4'
_space_group_name_Hall           'I -4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'

_cell_length_a                   30.0486(13)
_cell_length_b                   30.0486(13)
_cell_length_c                   19.3054(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     17431.2(17)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9660
_cell_measurement_theta_min      2.28
_cell_measurement_theta_max      28.33

_exptl_crystal_description       block
_exptl_crystal_colour            blue-violet
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_F_000             7888
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    2.288
_shelx_estimated_absorpt_T_min   0.829
_shelx_estimated_absorpt_T_max   0.860
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.623
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   'SADABS-2016/2 - Bruker AXS'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.72932
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'ALBA XALOC beamline'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'MD2M - Maatel + Dectris PILATUS 6M'
_diffrn_measurement_method       'ω rotation at various κ'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            118618
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         0.983
_diffrn_reflns_theta_max         27.488
_diffrn_reflns_theta_full        27.488
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             18367
_reflns_number_gt                15958
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.932
_reflns_Friedel_fraction_max     0.985
_reflns_Friedel_fraction_full    0.985

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Global Phasing autoPROC package'
_computing_cell_refinement       'Bruker SAINT v8.38a'
_computing_data_reduction        'Bruker SAINT v8.38a'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;All non-hydrogens were refined anisotropically. 
 Hydrogens were placed geometrically on their carrier atom and refined with 
 a riding model, including those on the pyrazole N (AFIX 43), as no clear
 electron density was present to allow proper free refinement. Hydrogens on the
 lattice water molecules could not be found and are omitted in the structural
 model but included in the formula.
 One of the Br anion is disordered over three positions with relative occupancies
 refining to 0.39:0.39:0.22 (Br3A:B:C). The BF4 ion was refined with 1,2 and 1,3
 distance restraints. Displacement parameters restraints were used to refine the 
 lattice water and methanol molecules. 
 At the end of the refinement there remained void spaces with only
 weak electron density peaks (except at a special position, where a 4 e peak
 was present but could not be included in the model in a sensible and converging
 manner). Analysis with PLATON/SQUEEZE (see below for details) gave 
 two large voids of 1562 cubic angstrom and two voids of 520 cubic angstroms
 per cell, with 515 and 174 electrons respectively. Although high in
 terms of electron content, these figures could correspond to 
 respectively 28 and 9 diffuse methanol molecules per void, for a total
 of 72 per cell, 9 per formula unit. As crystals were freshly taken out of
 their solution, this remains reasonable, and was therefore reflected in the 
 reported formula, calculated density, mu etc. Refinement with the squeezed data
 resulted in an improvement in R1 of ca. 2%.

# SQUEEZE RESULTS (Version = 180518)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.000  0.000  0.003      1562       515 ' '
   2  0.000  0.500  0.625       520       174 ' '
   3  0.120  0.802  0.286        12         0 ' '
   4  0.129  0.738  0.337         9        -2 ' '
   5  0.191  0.757  0.295         8         4 ' '
   6  0.198  0.120  0.714        12         0 ' '
   7  0.243  0.372  0.168        10        -3 ' '
   8  0.244  0.187  0.703         9         3 ' '
   9  0.264  0.125  0.660         8        -2 ' '
  10  0.257  0.309  0.206         8         4 ' '
  11  0.500  0.500  0.957      1562       515 ' '
  12  0.306  0.381  0.217        11         0 ' '
  13  0.314  0.744  0.797         9         3 ' '
  14  0.380  0.698  0.786        12         0 ' '
  15  0.500  0.000  0.379       520       174 ' '
  16  0.375  0.764  0.840         8        -2 ' '
  17  0.620  0.302  0.786        12         0 ' '
  18  0.629  0.238  0.837         9        -2 ' '
  19  0.691  0.257  0.795         8         4 ' '
  20  0.698  0.620  0.214        12         0 ' '
  21  0.743  0.872  0.668        10        -3 ' '
  22  0.744  0.687  0.203         9         3 ' '
  23  0.764  0.625  0.160         8        -2 ' '
  24  0.757  0.809  0.706         8         4 ' '
  25  0.806  0.881  0.717        11         0 ' '
  26  0.814  0.244  0.297         9         3 ' '
  27  0.880  0.198  0.286        12         0 ' '
  28  0.875  0.264  0.340         8        -2 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           ?,SQUEEZE
;

_vrf_FORMU01_MI7                 
;
PROBLEM: There is a discrepancy between the atom counts in the
            _chemical_formula_sum and the formula from the _atom_site* data.
            Atom count from _chemical_formula_sum:C76 H98 B1 Br3 F4 N18 Ni2 O15
            Atom count from the _atom_site data:  C67 H52 B1 Br3 F4 N18 Ni2 O6      
RESPONSE: PLATON/SQUEEZE has been used to analyse and take into account
the diffuse solvent content, for a total of 9 addition methanol molecules 
per formula unit. Also, hydrogens on the lattice water molecule could not be
found and are omitted in the structural model, but included in the formula. 
This has been reflected in the formula, giving rise to this discrepancy 
between the formula from the atom list and that reported.
;

_vrf_PLAT306_MI7                 
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?)      
RESPONSE: Hydrogens on the lattice water molecule could not be found and 
are indeed omitted in the structural model.
;

_vrf_PLAT973_MI7                 
;
PROBLEM: Check Calcd Positive Resid. Density on       Ni1       1.93 eA-3      
RESPONSE: The 2 largest remaining electron density are at or in the vicinity of 
both Ni sites, which could be due to un-ideal absorption corrections.
;

_vrf_PLAT971_MI7                 
;
PROBLEM: Check Calcd Resid. Dens.  0.20Ang From Ni2             1.83 eA-3      
RESPONSE: The 2 largest remaining electron density are at or in the vicinity of 
both Ni sites, which could be due to un-ideal absorption corrections.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2507P)²+0.4600P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 6719 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.111(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         18367
_refine_ls_number_parameters     930
_refine_ls_number_restraints     52
_refine_ls_R_factor_all          0.1068
_refine_ls_R_factor_gt           0.0991
_refine_ls_wR_factor_ref         0.2911
_refine_ls_wR_factor_gt          0.2786
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.28431(3) 0.86446(4) 0.35931(6) 0.0414(3) Uani 1 1 d . . . . .
Ni2 Ni 0.51695(4) 0.73728(4) 0.65072(6) 0.0452(3) Uani 1 1 d . . . . .
N1 N 0.2156(2) 0.8619(3) 0.3865(5) 0.0518(18) Uani 1 1 d . . . . .
N2 N 0.2783(2) 0.8009(2) 0.4009(4) 0.0409(14) Uani 1 1 d . . . . .
N3 N 0.3054(2) 0.7659(3) 0.4170(4) 0.0429(15) Uani 1 1 d . . . . .
H3B H 0.334406 0.765664 0.411068 0.052 Uiso 1 1 calc R U . . .
N4 N 0.4267(3) 0.7012(3) 0.5840(5) 0.0513(19) Uani 1 1 d . . . . .
H4B H 0.410616 0.725477 0.588849 0.062 Uiso 1 1 calc R U . . .
N5 N 0.4689(3) 0.6974(3) 0.6024(5) 0.0506(18) Uani 1 1 d . . . . .
N6 N 0.5527(3) 0.6776(3) 0.6333(5) 0.0515(18) Uani 1 1 d . . . . .
N7 N 0.2754(3) 0.8425(3) 0.2569(4) 0.0491(17) Uani 1 1 d . . . . .
N8 N 0.3495(2) 0.8558(2) 0.3261(4) 0.0429(15) Uani 1 1 d . . . . .
N9 N 0.3910(2) 0.8592(3) 0.3505(4) 0.0432(15) Uani 1 1 d . . . . .
H9A H 0.397670 0.866514 0.393410 0.052 Uiso 1 1 calc R U . . .
N10 N 0.5189(2) 0.7806(2) 0.4975(4) 0.0392(14) Uani 1 1 d . . . . .
H10B H 0.496096 0.766479 0.479313 0.047 Uiso 1 1 calc R U . . .
N11 N 0.5355(2) 0.7725(2) 0.5623(4) 0.0400(14) Uani 1 1 d . . . . .
N12 N 0.5744(3) 0.7730(3) 0.6834(5) 0.0523(18) Uani 1 1 d . . . . .
N13 N 0.2787(2) 0.9322(3) 0.3289(5) 0.0481(17) Uani 1 1 d . . . . .
N14 N 0.3027(3) 0.8986(3) 0.4493(4) 0.0480(17) Uani 1 1 d . . . . .
N15 N 0.3219(3) 0.8889(3) 0.5093(4) 0.0434(15) Uani 1 1 d . . . . .
H15A H 0.326934 0.861697 0.524203 0.052 Uiso 1 1 calc R U . . .
N16 N 0.4542(3) 0.8234(3) 0.6595(4) 0.0458(16) Uani 1 1 d . . . . .
H16B H 0.456464 0.831825 0.615987 0.055 Uiso 1 1 calc R U . . .
N17 N 0.4735(3) 0.7872(3) 0.6850(4) 0.0496(17) Uani 1 1 d . . . . .
N18 N 0.5016(3) 0.7170(4) 0.7543(5) 0.057(2) Uani 1 1 d . . . . .
C1 C 0.1856(4) 0.8956(5) 0.3803(9) 0.072(3) Uani 1 1 d . . . . .
H1A H 0.194101 0.923135 0.360046 0.087 Uiso 1 1 calc R U . . .
C2 C 0.1408(4) 0.8891(6) 0.4046(9) 0.082(4) Uani 1 1 d . . . . .
H2A H 0.120513 0.913361 0.404380 0.099 Uiso 1 1 calc R U . . .
C3 C 0.1275(4) 0.8498(7) 0.4274(11) 0.095(5) Uani 1 1 d . . . . .
H3A H 0.097945 0.846550 0.444330 0.114 Uiso 1 1 calc R U . . .
C4 C 0.1575(4) 0.8105(7) 0.4271(10) 0.092(5) Uani 1 1 d . . . . .
H4A H 0.147743 0.781010 0.436464 0.111 Uiso 1 1 calc R U . . .
C5 C 0.2010(3) 0.8212(4) 0.4117(6) 0.055(2) Uani 1 1 d . . . . .
C6 C 0.2370(3) 0.7884(3) 0.4176(5) 0.0451(18) Uani 1 1 d . . . . .
C7 C 0.2369(3) 0.7441(4) 0.4428(5) 0.050(2) Uani 1 1 d . . . . .
H7A H 0.212025 0.726653 0.456280 0.061 Uiso 1 1 calc R U . . .
C8 C 0.2816(3) 0.7318(3) 0.4432(5) 0.0441(18) Uani 1 1 d . . . . .
C9 C 0.3034(3) 0.6927(3) 0.4710(5) 0.0441(18) Uani 1 1 d . . . . .
C10 C 0.2808(3) 0.6518(3) 0.4773(6) 0.052(2) Uani 1 1 d . . . . .
H10A H 0.251765 0.648879 0.458358 0.062 Uiso 1 1 calc R U . . .
C11 C 0.2998(4) 0.6158(4) 0.5104(7) 0.063(3) Uani 1 1 d . . . . .
H11A H 0.283296 0.589183 0.516800 0.075 Uiso 1 1 calc R U . . .
C12 C 0.3429(4) 0.6187(3) 0.5341(7) 0.058(2) Uani 1 1 d . . . . .
H12A H 0.356589 0.593381 0.554560 0.069 Uiso 1 1 calc R U . . .
C13 C 0.3667(4) 0.6584(3) 0.5284(6) 0.051(2) Uani 1 1 d . . . . .
C14 C 0.3455(3) 0.6947(3) 0.4970(5) 0.0420(16) Uani 1 1 d . . . . .
H14A H 0.361302 0.722031 0.493581 0.050 Uiso 1 1 calc R U . . .
C15 C 0.4116(3) 0.6625(3) 0.5565(5) 0.0469(19) Uani 1 1 d . . . . .
C16 C 0.4456(3) 0.6315(3) 0.5624(6) 0.049(2) Uani 1 1 d . . . . .
H16A H 0.444799 0.600893 0.550218 0.059 Uiso 1 1 calc R U . . .
C17 C 0.4817(3) 0.6555(3) 0.5907(6) 0.052(2) Uani 1 1 d . . . . .
C18 C 0.5273(4) 0.6427(4) 0.6077(7) 0.058(2) Uani 1 1 d . . . . .
C19 C 0.5433(5) 0.6024(4) 0.5973(9) 0.074(3) Uani 1 1 d . . . . .
H19A H 0.523295 0.579806 0.582482 0.089 Uiso 1 1 calc R U . . .
C20 C 0.5875(6) 0.5911(5) 0.6068(14) 0.102(6) Uani 1 1 d . . . . .
H20A H 0.599499 0.563140 0.593602 0.123 Uiso 1 1 calc R U . . .
C21 C 0.6149(5) 0.6271(5) 0.6398(11) 0.092(5) Uani 1 1 d . . . . .
H21A H 0.644833 0.621751 0.653131 0.110 Uiso 1 1 calc R U . . .
C22 C 0.5953(3) 0.6684(4) 0.6503(6) 0.057(2) Uani 1 1 d . . . . .
H22A H 0.612703 0.691287 0.670570 0.068 Uiso 1 1 calc R U . . .
C23 C 0.2361(4) 0.8343(5) 0.2229(7) 0.067(3) Uani 1 1 d . . . . .
H23A H 0.209087 0.837815 0.247999 0.081 Uiso 1 1 calc R U . . .
C24 C 0.2335(5) 0.8215(7) 0.1553(8) 0.084(4) Uani 1 1 d . . . . .
H24A H 0.205479 0.817078 0.133702 0.101 Uiso 1 1 calc R U . . .
C25 C 0.2723(5) 0.8150(7) 0.1191(8) 0.089(5) Uani 1 1 d . . . . .
H25A H 0.271316 0.806347 0.071747 0.106 Uiso 1 1 calc R U . . .
C26 C 0.3131(4) 0.8212(5) 0.1522(6) 0.067(3) Uani 1 1 d . . . . .
H26A H 0.340227 0.815631 0.128526 0.080 Uiso 1 1 calc R U . . .
C27 C 0.3132(3) 0.8360(4) 0.2210(5) 0.0483(19) Uani 1 1 d . . . . .
C28 C 0.3544(3) 0.8444(3) 0.2582(5) 0.0409(16) Uani 1 1 d . . . . .
C29 C 0.3988(3) 0.8416(3) 0.2417(5) 0.0463(19) Uani 1 1 d . . . . .
H29A H 0.411249 0.834904 0.197716 0.056 Uiso 1 1 calc R U . . .
C30 C 0.4210(3) 0.8502(3) 0.3012(5) 0.0465(18) Uani 1 1 d . . . . .
C31 C 0.4699(3) 0.8505(3) 0.3186(5) 0.0437(17) Uani 1 1 d . . . . .
C32 C 0.5014(3) 0.8705(4) 0.2730(6) 0.053(2) Uani 1 1 d . . . . .
H32A H 0.492184 0.883864 0.230723 0.063 Uiso 1 1 calc R U . . .
C33 C 0.5451(3) 0.8700(4) 0.2917(6) 0.059(3) Uani 1 1 d . . . . .
H33A H 0.566584 0.882095 0.260963 0.071 Uiso 1 1 calc R U . . .
C34 C 0.5591(3) 0.8524(4) 0.3546(7) 0.057(2) Uani 1 1 d . . . . .
H34A H 0.589497 0.854333 0.367878 0.069 Uiso 1 1 calc R U . . .
C35 C 0.5284(3) 0.8319(3) 0.3976(5) 0.0448(18) Uani 1 1 d . . . . .
C36 C 0.4829(3) 0.8309(3) 0.3797(5) 0.0420(17) Uani 1 1 d . . . . .
H36A H 0.461777 0.817014 0.409228 0.050 Uiso 1 1 calc R U . . .
C37 C 0.5420(3) 0.8132(3) 0.4651(5) 0.0458(18) Uani 1 1 d . . . . .
C38 C 0.5760(3) 0.8266(3) 0.5098(5) 0.0470(19) Uani 1 1 d . . . . .
H38A H 0.598269 0.848431 0.501607 0.056 Uiso 1 1 calc R U . . .
C39 C 0.5699(3) 0.8003(3) 0.5701(5) 0.0458(18) Uani 1 1 d . . . . .
C40 C 0.5934(3) 0.7989(3) 0.6362(6) 0.0478(19) Uani 1 1 d . . . . .
C41 C 0.6328(3) 0.8221(3) 0.6491(7) 0.058(3) Uani 1 1 d . . . . .
H41A H 0.645754 0.840093 0.614029 0.070 Uiso 1 1 calc R U . . .
C42 C 0.6523(4) 0.8185(4) 0.7126(8) 0.068(3) Uani 1 1 d . . . . .
H42A H 0.679220 0.834002 0.722158 0.081 Uiso 1 1 calc R U . . .
C43 C 0.6329(5) 0.7925(5) 0.7625(8) 0.076(3) Uani 1 1 d . . . . .
H43A H 0.645954 0.790468 0.807215 0.091 Uiso 1 1 calc R U . . .
C44 C 0.5939(4) 0.7690(5) 0.7474(6) 0.061(3) Uani 1 1 d . . . . .
H44A H 0.580850 0.750335 0.781469 0.074 Uiso 1 1 calc R U . . .
C45 C 0.2635(4) 0.9466(4) 0.2669(6) 0.061(3) Uani 1 1 d . . . . .
H45A H 0.260114 0.925714 0.230363 0.074 Uiso 1 1 calc R U . . .
C46 C 0.2529(4) 0.9901(4) 0.2551(7) 0.063(3) Uani 1 1 d . . . . .
H46A H 0.242020 0.999065 0.211103 0.076 Uiso 1 1 calc R U . . .
C47 C 0.2585(4) 1.0229(4) 0.3105(8) 0.068(3) Uani 1 1 d . . . . .
H47A H 0.250600 1.053260 0.304239 0.082 Uiso 1 1 calc R U . . .
C48 C 0.2757(4) 1.0075(4) 0.3723(7) 0.063(3) Uani 1 1 d . . . . .
H48A H 0.281384 1.027503 0.409412 0.076 Uiso 1 1 calc R U . . .
C49 C 0.2849(3) 0.9613(3) 0.3795(6) 0.051(2) Uani 1 1 d . . . . .
C50 C 0.3022(3) 0.9423(3) 0.4444(6) 0.0476(19) Uani 1 1 d . . . . .
C51 C 0.3205(3) 0.9619(3) 0.5036(6) 0.052(2) Uani 1 1 d . . . . .
H51A H 0.324015 0.992645 0.513833 0.062 Uiso 1 1 calc R U . . .
C52 C 0.3325(3) 0.9254(3) 0.5439(5) 0.0476(19) Uani 1 1 d . . . . .
C53 C 0.3566(4) 0.9248(3) 0.6101(5) 0.051(2) Uani 1 1 d . . . . .
C54 C 0.3534(5) 0.9608(4) 0.6587(6) 0.064(3) Uani 1 1 d . . . . .
H54A H 0.335162 0.985914 0.649453 0.076 Uiso 1 1 calc R U . . .
C55 C 0.3776(5) 0.9578(4) 0.7195(7) 0.067(3) Uani 1 1 d . . . . .
H55A H 0.376768 0.982266 0.750624 0.081 Uiso 1 1 calc R U . . .
C56 C 0.4025(4) 0.9219(4) 0.7370(6) 0.064(3) Uani 1 1 d . . . . .
H56A H 0.417574 0.921172 0.780324 0.077 Uiso 1 1 calc R U . . .
C57 C 0.4062(3) 0.8857(4) 0.6914(6) 0.053(2) Uani 1 1 d . . . . .
C58 C 0.3817(3) 0.8877(3) 0.6284(5) 0.051(2) Uani 1 1 d . . . . .
H58A H 0.382634 0.862981 0.597786 0.061 Uiso 1 1 calc R U . . .
C59 C 0.4309(3) 0.8457(3) 0.7070(5) 0.0488(19) Uani 1 1 d . . . . .
C60 C 0.4370(3) 0.8233(4) 0.7697(5) 0.051(2) Uani 1 1 d . . . . .
H60A H 0.426167 0.831346 0.814226 0.061 Uiso 1 1 calc R U . . .
C61 C 0.4631(3) 0.7856(3) 0.7511(5) 0.0477(19) Uani 1 1 d . . . . .
C62 C 0.4786(3) 0.7465(4) 0.7904(6) 0.055(2) Uani 1 1 d . . . . .
C63 C 0.4689(4) 0.7431(5) 0.8616(7) 0.068(3) Uani 1 1 d . . . . .
H63A H 0.451989 0.765488 0.884416 0.082 Uiso 1 1 calc R U . . .
C64 C 0.4841(5) 0.7073(6) 0.8969(8) 0.081(4) Uani 1 1 d . . . . .
H64A H 0.479393 0.704186 0.945313 0.097 Uiso 1 1 calc R U . . .
C65 C 0.5081(5) 0.6737(5) 0.8575(9) 0.077(4) Uani 1 1 d . . . . .
H65A H 0.518502 0.647488 0.879758 0.093 Uiso 1 1 calc R U . . .
C66 C 0.5156(4) 0.6800(5) 0.7888(8) 0.070(3) Uani 1 1 d . . . . .
H66A H 0.531235 0.657746 0.763775 0.083 Uiso 1 1 calc R U . . .
Br1 Br 0.40211(5) 0.80157(5) 0.50648(8) 0.0747(4) Uani 1 1 d . . . . .
Br2 Br 0.39336(5) 0.73400(5) 0.32262(9) 0.0775(4) Uani 1 1 d . . . . .
Br3A Br 0.47428(17) 0.70009(17) 0.4128(3) 0.0970(14) Uani 0.39 1 d . . P A 1
Br3B Br 0.2893(2) 0.79644(14) 0.5888(2) 0.1034(17) Uani 0.39 1 d . . P B 2
Br3C Br 0.3449(3) 0.7906(3) 0.5933(5) 0.099(2) Uani 0.22 1 d . . P C 3
B1 B 0.3962(3) 0.8097(4) 0.9972(5) 0.060(3) Uani 1 1 d D . . . .
F1 F 0.4081(3) 0.8324(3) 1.0598(4) 0.081(2) Uani 1 1 d D . . . .
F2 F 0.3519(2) 0.8080(4) 0.9924(5) 0.089(3) Uani 1 1 d D . . . .
F3 F 0.4166(3) 0.8326(4) 0.9433(5) 0.094(3) Uani 1 1 d D . . . .
F4 F 0.4158(4) 0.7676(3) 1.0010(5) 0.097(3) Uani 1 1 d D . . . .
O1W O 0.3598(7) 0.7541(5) 0.6757(10) 0.135(6) Uani 1 1 d . . . . .
O2W O 0.7260(19) 0.7179(19) 0.762(3) 0.27(2) Uani 1 1 d . U . . .
O3W O 0.3999(17) 0.6077(18) 0.728(3) 0.250(17) Uani 1 1 d . U . . .
O4W O 0.0134(11) 0.8656(11) 0.5473(18) 0.195(11) Uani 1 1 d . U . . .
O5W O 0.4266(5) 0.9252(7) 0.4483(8) 0.135(6) Uani 1 1 d . U . . .
O1S O 0.4815(8) 0.8779(8) 0.5463(12) 0.141(6) Uani 1 1 d . U . . .
H1S H 0.463988 0.882958 0.508462 0.211 Uiso 1 1 d R U . . .
C1S C 0.5039(10) 0.9095(8) 0.5716(15) 0.124(7) Uani 1 1 d . U . . .
H1S1 H 0.484839 0.935803 0.576657 0.187 Uiso 1 1 calc R U . . .
H1S2 H 0.528811 0.916519 0.540786 0.187 Uiso 1 1 calc R U . . .
H1S3 H 0.515355 0.900753 0.617147 0.187 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N8 2.076(8) . ?
Ni1 N2 2.080(8) . ?
Ni1 N14 2.092(8) . ?
Ni1 N7 2.101(9) . ?
Ni1 N13 2.125(8) . ?
Ni1 N1 2.131(8) . ?
Ni2 N11 2.085(8) . ?
Ni2 N5 2.096(9) . ?
Ni2 N17 2.096(8) . ?
Ni2 N6 2.117(9) . ?
Ni2 N12 2.128(8) . ?
Ni2 N18 2.141(9) . ?
N1 C1 1.362(14) . ?
N1 C5 1.387(14) . ?
N2 C6 1.337(11) . ?
N2 N3 1.364(11) . ?
N3 C8 1.348(12) . ?
N3 H3B 0.8800 . ?
N4 N5 1.322(11) . ?
N4 C15 1.356(13) . ?
N4 H4B 0.8800 . ?
N5 C17 1.336(14) . ?
N6 C22 1.350(13) . ?
N6 C18 1.387(15) . ?
N7 C27 1.345(13) . ?
N7 C23 1.373(13) . ?
N8 N9 1.337(10) . ?
N8 C28 1.363(12) . ?
N9 C30 1.341(13) . ?
N9 H9A 0.8800 . ?
N10 C37 1.352(12) . ?
N10 N11 1.367(11) . ?
N10 H10B 0.8800 . ?
N11 C39 1.337(12) . ?
N12 C40 1.326(15) . ?
N12 C44 1.372(14) . ?
N13 C49 1.324(15) . ?
N13 C45 1.351(14) . ?
N14 C50 1.315(13) . ?
N14 N15 1.328(12) . ?
N15 C52 1.322(13) . ?
N15 H15A 0.8800 . ?
N16 N17 1.329(12) . ?
N16 C59 1.333(13) . ?
N16 H16B 0.8800 . ?
N17 C61 1.314(14) . ?
N18 C62 1.325(17) . ?
N18 C66 1.361(16) . ?
C1 C2 1.439(19) . ?
C1 H1A 0.9500 . ?
C2 C3 1.32(3) . ?
C2 H2A 0.9500 . ?
C3 C4 1.49(3) . ?
C3 H3A 0.9500 . ?
C4 C5 1.380(17) . ?
C4 H4A 0.9500 . ?
C5 C6 1.467(13) . ?
C6 C7 1.417(15) . ?
C7 C8 1.391(13) . ?
C7 H7A 0.9500 . ?
C8 C9 1.449(14) . ?
C9 C14 1.363(12) . ?
C9 C10 1.412(12) . ?
C10 C11 1.379(16) . ?
C10 H10A 0.9500 . ?
C11 C12 1.375(16) . ?
C11 H11A 0.9500 . ?
C12 C13 1.397(13) . ?
C12 H12A 0.9500 . ?
C13 C14 1.401(13) . ?
C13 C15 1.457(15) . ?
C14 H14A 0.9500 . ?
C15 C16 1.388(13) . ?
C16 C17 1.411(15) . ?
C16 H16A 0.9500 . ?
C17 C18 1.463(15) . ?
C18 C19 1.317(18) . ?
C19 C20 1.38(2) . ?
C19 H19A 0.9500 . ?
C20 C21 1.50(3) . ?
C20 H20A 0.9500 . ?
C21 C22 1.388(19) . ?
C21 H21A 0.9500 . ?
C22 H22A 0.9500 . ?
C23 C24 1.36(2) . ?
C23 H23A 0.9500 . ?
C24 C25 1.37(2) . ?
C24 H24A 0.9500 . ?
C25 C26 1.396(19) . ?
C25 H25A 0.9500 . ?
C26 C27 1.401(16) . ?
C26 H26A 0.9500 . ?
C27 C28 1.454(13) . ?
C28 C29 1.373(13) . ?
C29 C30 1.353(15) . ?
C29 H29A 0.9500 . ?
C30 C31 1.507(12) . ?
C31 C36 1.376(14) . ?
C31 C32 1.426(12) . ?
C32 C33 1.361(15) . ?
C32 H32A 0.9500 . ?
C33 C34 1.389(17) . ?
C33 H33A 0.9500 . ?
C34 C35 1.386(14) . ?
C34 H34A 0.9500 . ?
C35 C36 1.410(11) . ?
C35 C37 1.475(14) . ?
C36 H36A 0.9500 . ?
C37 C38 1.398(13) . ?
C38 C39 1.419(14) . ?
C38 H38A 0.9500 . ?
C39 C40 1.460(15) . ?
C40 C41 1.395(13) . ?
C41 C42 1.364(19) . ?
C41 H41A 0.9500 . ?
C42 C43 1.37(2) . ?
C42 H42A 0.9500 . ?
C43 C44 1.401(19) . ?
C43 H43A 0.9500 . ?
C44 H44A 0.9500 . ?
C45 C46 1.365(17) . ?
C45 H45A 0.9500 . ?
C46 C47 1.46(2) . ?
C46 H46A 0.9500 . ?
C47 C48 1.380(19) . ?
C47 H47A 0.9500 . ?
C48 C49 1.423(15) . ?
C48 H48A 0.9500 . ?
C49 C50 1.473(15) . ?
C50 C51 1.399(15) . ?
C51 C52 1.393(15) . ?
C51 H51A 0.9500 . ?
C52 C53 1.468(15) . ?
C53 C58 1.392(14) . ?
C53 C54 1.435(14) . ?
C54 C55 1.383(19) . ?
C54 H54A 0.9500 . ?
C55 C56 1.36(2) . ?
C55 H55A 0.9500 . ?
C56 C57 1.402(15) . ?
C56 H56A 0.9500 . ?
C57 C58 1.422(15) . ?
C57 C59 1.447(15) . ?
C58 H58A 0.9500 . ?
C59 C60 1.396(15) . ?
C60 C61 1.426(15) . ?
C60 H60A 0.9500 . ?
C61 C62 1.472(15) . ?
C62 C63 1.409(18) . ?
C63 C64 1.35(2) . ?
C63 H63A 0.9500 . ?
C64 C65 1.45(3) . ?
C64 H64A 0.9500 . ?
C65 C66 1.36(2) . ?
C65 H65A 0.9500 . ?
C66 H66A 0.9500 . ?
Br1 Br3C 2.423(10) . ?
Br3C O1W 1.98(2) . ?
B1 F2 1.336(12) . ?
B1 F3 1.389(13) . ?
B1 F4 1.397(12) . ?
B1 F1 1.433(12) . ?
O1S C1S 1.26(4) . ?
O1S H1S 0.9123 . ?
C1S H1S1 0.9800 . ?
C1S H1S2 0.9800 . ?
C1S H1S3 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N8 Ni1 N2 94.9(3) . . ?
N8 Ni1 N14 93.9(3) . . ?
N2 Ni1 N14 98.8(3) . . ?
N8 Ni1 N7 77.9(3) . . ?
N2 Ni1 N7 93.6(3) . . ?
N14 Ni1 N7 165.7(3) . . ?
N8 Ni1 N13 96.3(3) . . ?
N2 Ni1 N13 168.4(3) . . ?
N14 Ni1 N13 77.3(3) . . ?
N7 Ni1 N13 91.8(3) . . ?
N8 Ni1 N1 170.0(3) . . ?
N2 Ni1 N1 77.8(3) . . ?
N14 Ni1 N1 94.0(3) . . ?
N7 Ni1 N1 95.6(3) . . ?
N13 Ni1 N1 91.5(3) . . ?
N11 Ni2 N5 96.3(3) . . ?
N11 Ni2 N17 93.5(3) . . ?
N5 Ni2 N17 96.9(3) . . ?
N11 Ni2 N6 99.5(3) . . ?
N5 Ni2 N6 78.1(3) . . ?
N17 Ni2 N6 166.5(4) . . ?
N11 Ni2 N12 76.7(3) . . ?
N5 Ni2 N12 168.3(4) . . ?
N17 Ni2 N12 92.9(3) . . ?
N6 Ni2 N12 93.6(3) . . ?
N11 Ni2 N18 165.2(4) . . ?
N5 Ni2 N18 96.0(4) . . ?
N17 Ni2 N18 77.0(4) . . ?
N6 Ni2 N18 90.9(4) . . ?
N12 Ni2 N18 92.3(4) . . ?
C1 N1 C5 118.5(9) . . ?
C1 N1 Ni1 126.4(9) . . ?
C5 N1 Ni1 115.1(6) . . ?
C6 N2 N3 106.4(7) . . ?
C6 N2 Ni1 115.6(6) . . ?
N3 N2 Ni1 138.0(5) . . ?
C8 N3 N2 110.8(7) . . ?
C8 N3 H3B 124.6 . . ?
N2 N3 H3B 124.6 . . ?
N5 N4 C15 110.7(8) . . ?
N5 N4 H4B 124.7 . . ?
C15 N4 H4B 124.7 . . ?
N4 N5 C17 108.1(8) . . ?
N4 N5 Ni2 137.0(7) . . ?
C17 N5 Ni2 114.6(7) . . ?
C22 N6 C18 116.8(9) . . ?
C22 N6 Ni2 128.0(8) . . ?
C18 N6 Ni2 114.8(7) . . ?
C27 N7 C23 117.0(9) . . ?
C27 N7 Ni1 115.0(6) . . ?
C23 N7 Ni1 128.0(8) . . ?
N9 N8 C28 104.9(7) . . ?
N9 N8 Ni1 139.5(6) . . ?
C28 N8 Ni1 115.6(6) . . ?
N8 N9 C30 111.2(8) . . ?
N8 N9 H9A 124.4 . . ?
C30 N9 H9A 124.4 . . ?
C37 N10 N11 111.5(7) . . ?
C37 N10 H10B 124.3 . . ?
N11 N10 H10B 124.3 . . ?
C39 N11 N10 105.9(7) . . ?
C39 N11 Ni2 115.5(6) . . ?
N10 N11 Ni2 137.9(5) . . ?
C40 N12 C44 119.0(9) . . ?
C40 N12 Ni2 116.2(7) . . ?
C44 N12 Ni2 124.7(8) . . ?
C49 N13 C45 119.3(9) . . ?
C49 N13 Ni1 114.7(7) . . ?
C45 N13 Ni1 125.3(8) . . ?
C50 N14 N15 106.7(8) . . ?
C50 N14 Ni1 115.3(7) . . ?
N15 N14 Ni1 137.1(6) . . ?
C52 N15 N14 111.3(8) . . ?
C52 N15 H15A 124.3 . . ?
N14 N15 H15A 124.3 . . ?
N17 N16 C59 112.7(8) . . ?
N17 N16 H16B 123.7 . . ?
C59 N16 H16B 123.7 . . ?
C61 N17 N16 106.6(8) . . ?
C61 N17 Ni2 115.4(7) . . ?
N16 N17 Ni2 137.9(7) . . ?
C62 N18 C66 116.8(11) . . ?
C62 N18 Ni2 114.4(7) . . ?
C66 N18 Ni2 128.5(10) . . ?
N1 C1 C2 119.4(13) . . ?
N1 C1 H1A 120.3 . . ?
C2 C1 H1A 120.3 . . ?
C3 C2 C1 120.9(14) . . ?
C3 C2 H2A 119.6 . . ?
C1 C2 H2A 119.6 . . ?
C2 C3 C4 121.6(13) . . ?
C2 C3 H3A 119.2 . . ?
C4 C3 H3A 119.2 . . ?
C5 C4 C3 113.0(16) . . ?
C5 C4 H4A 123.5 . . ?
C3 C4 H4A 123.5 . . ?
C4 C5 N1 125.5(11) . . ?
C4 C5 C6 121.6(12) . . ?
N1 C5 C6 112.8(8) . . ?
N2 C6 C7 110.3(8) . . ?
N2 C6 C5 118.4(8) . . ?
C7 C6 C5 131.2(8) . . ?
C8 C7 C6 104.5(7) . . ?
C8 C7 H7A 127.8 . . ?
C6 C7 H7A 127.8 . . ?
N3 C8 C7 108.0(9) . . ?
N3 C8 C9 121.0(8) . . ?
C7 C8 C9 130.8(8) . . ?
C14 C9 C10 117.0(9) . . ?
C14 C9 C8 121.4(8) . . ?
C10 C9 C8 121.4(8) . . ?
C11 C10 C9 121.6(8) . . ?
C11 C10 H10A 119.2 . . ?
C9 C10 H10A 119.2 . . ?
C12 C11 C10 119.7(9) . . ?
C12 C11 H11A 120.2 . . ?
C10 C11 H11A 120.1 . . ?
C11 C12 C13 120.6(10) . . ?
C11 C12 H12A 119.7 . . ?
C13 C12 H12A 119.7 . . ?
C12 C13 C14 117.8(10) . . ?
C12 C13 C15 121.0(9) . . ?
C14 C13 C15 121.1(8) . . ?
C9 C14 C13 123.2(8) . . ?
C9 C14 H14A 118.4 . . ?
C13 C14 H14A 118.4 . . ?
N4 C15 C16 107.2(9) . . ?
N4 C15 C13 121.8(8) . . ?
C16 C15 C13 131.0(9) . . ?
C15 C16 C17 104.8(8) . . ?
C15 C16 H16A 127.6 . . ?
C17 C16 H16A 127.6 . . ?
N5 C17 C16 109.1(8) . . ?
N5 C17 C18 118.7(10) . . ?
C16 C17 C18 132.3(10) . . ?
C19 C18 N6 123.3(11) . . ?
C19 C18 C17 123.3(12) . . ?
N6 C18 C17 113.3(9) . . ?
C18 C19 C20 123.6(15) . . ?
C18 C19 H19A 118.2 . . ?
C20 C19 H19A 118.2 . . ?
C19 C20 C21 114.0(14) . . ?
C19 C20 H20A 123.0 . . ?
C21 C20 H20A 123.0 . . ?
C22 C21 C20 118.2(12) . . ?
C22 C21 H21A 120.9 . . ?
C20 C21 H21A 120.9 . . ?
N6 C22 C21 123.4(12) . . ?
N6 C22 H22A 118.3 . . ?
C21 C22 H22A 118.3 . . ?
C24 C23 N7 123.8(12) . . ?
C24 C23 H23A 118.1 . . ?
N7 C23 H23A 118.1 . . ?
C23 C24 C25 118.8(12) . . ?
C23 C24 H24A 120.6 . . ?
C25 C24 H24A 120.6 . . ?
C24 C25 C26 119.5(13) . . ?
C24 C25 H25A 120.2 . . ?
C26 C25 H25A 120.2 . . ?
C25 C26 C27 118.6(12) . . ?
C25 C26 H26A 120.7 . . ?
C27 C26 H26A 120.7 . . ?
N7 C27 C26 122.2(9) . . ?
N7 C27 C28 116.1(9) . . ?
C26 C27 C28 121.7(9) . . ?
N8 C28 C29 110.2(8) . . ?
N8 C28 C27 115.2(8) . . ?
C29 C28 C27 134.6(9) . . ?
C30 C29 C28 105.7(9) . . ?
C30 C29 H29A 127.1 . . ?
C28 C29 H29A 127.1 . . ?
N9 C30 C29 108.0(8) . . ?
N9 C30 C31 119.8(9) . . ?
C29 C30 C31 132.2(9) . . ?
C36 C31 C32 121.4(8) . . ?
C36 C31 C30 117.8(8) . . ?
C32 C31 C30 120.8(8) . . ?
C33 C32 C31 118.1(9) . . ?
C33 C32 H32A 121.0 . . ?
C31 C32 H32A 121.0 . . ?
C32 C33 C34 122.0(9) . . ?
C32 C33 H33A 119.0 . . ?
C34 C33 H33A 119.0 . . ?
C35 C34 C33 119.4(9) . . ?
C35 C34 H34A 120.3 . . ?
C33 C34 H34A 120.3 . . ?
C34 C35 C36 120.5(9) . . ?
C34 C35 C37 121.0(8) . . ?
C36 C35 C37 118.4(8) . . ?
C31 C36 C35 118.5(8) . . ?
C31 C36 H36A 120.8 . . ?
C35 C36 H36A 120.8 . . ?
N10 C37 C38 107.3(9) . . ?
N10 C37 C35 122.9(8) . . ?
C38 C37 C35 129.5(9) . . ?
C37 C38 C39 104.5(8) . . ?
C37 C38 H38A 127.7 . . ?
C39 C38 H38A 127.7 . . ?
N11 C39 C38 110.8(8) . . ?
N11 C39 C40 117.0(9) . . ?
C38 C39 C40 132.1(8) . . ?
N12 C40 C41 122.4(10) . . ?
N12 C40 C39 114.2(8) . . ?
C41 C40 C39 123.4(10) . . ?
C42 C41 C40 119.1(12) . . ?
C42 C41 H41A 120.5 . . ?
C40 C41 H41A 120.5 . . ?
C41 C42 C43 119.5(11) . . ?
C41 C42 H42A 120.2 . . ?
C43 C42 H42A 120.2 . . ?
C42 C43 C44 119.8(12) . . ?
C42 C43 H43A 120.1 . . ?
C44 C43 H43A 120.1 . . ?
N12 C44 C43 120.1(13) . . ?
N12 C44 H44A 120.0 . . ?
C43 C44 H44A 120.0 . . ?
N13 C45 C46 122.2(12) . . ?
N13 C45 H45A 118.9 . . ?
C46 C45 H45A 118.9 . . ?
C45 C46 C47 119.8(11) . . ?
C45 C46 H46A 120.1 . . ?
C47 C46 H46A 120.1 . . ?
C48 C47 C46 116.7(11) . . ?
C48 C47 H47A 121.7 . . ?
C46 C47 H47A 121.7 . . ?
C47 C48 C49 118.9(12) . . ?
C47 C48 H48A 120.5 . . ?
C49 C48 H48A 120.5 . . ?
N13 C49 C48 123.1(10) . . ?
N13 C49 C50 114.9(9) . . ?
C48 C49 C50 122.0(11) . . ?
N14 C50 C51 110.9(9) . . ?
N14 C50 C49 116.8(9) . . ?
C51 C50 C49 132.2(9) . . ?
C52 C51 C50 103.1(8) . . ?
C52 C51 H51A 128.5 . . ?
C50 C51 H51A 128.5 . . ?
N15 C52 C51 108.0(9) . . ?
N15 C52 C53 123.3(9) . . ?
C51 C52 C53 128.5(9) . . ?
C58 C53 C54 118.3(9) . . ?
C58 C53 C52 119.8(9) . . ?
C54 C53 C52 121.8(9) . . ?
C55 C54 C53 118.1(10) . . ?
C55 C54 H54A 121.0 . . ?
C53 C54 H54A 121.0 . . ?
C56 C55 C54 123.6(10) . . ?
C56 C55 H55A 118.2 . . ?
C54 C55 H55A 118.2 . . ?
C55 C56 C57 120.1(11) . . ?
C55 C56 H56A 119.9 . . ?
C57 C56 H56A 119.9 . . ?
C56 C57 C58 117.7(10) . . ?
C56 C57 C59 123.6(10) . . ?
C58 C57 C59 118.6(9) . . ?
C53 C58 C57 122.0(9) . . ?
C53 C58 H58A 119.0 . . ?
C57 C58 H58A 119.0 . . ?
N16 C59 C60 106.7(9) . . ?
N16 C59 C57 123.0(10) . . ?
C60 C59 C57 130.4(10) . . ?
C59 C60 C61 103.7(9) . . ?
C59 C60 H60A 128.2 . . ?
C61 C60 H60A 128.2 . . ?
N17 C61 C60 110.3(9) . . ?
N17 C61 C62 117.1(9) . . ?
C60 C61 C62 132.6(10) . . ?
N18 C62 C63 124.9(11) . . ?
N18 C62 C61 115.3(10) . . ?
C63 C62 C61 119.8(11) . . ?
C64 C63 C62 118.6(14) . . ?
C64 C63 H63A 120.7 . . ?
C62 C63 H63A 120.7 . . ?
C63 C64 C65 117.2(13) . . ?
C63 C64 H64A 121.4 . . ?
C65 C64 H64A 121.4 . . ?
C66 C65 C64 119.7(12) . . ?
C66 C65 H65A 120.2 . . ?
C64 C65 H65A 120.2 . . ?
C65 C66 N18 122.7(15) . . ?
C65 C66 H66A 118.6 . . ?
N18 C66 H66A 118.6 . . ?
O1W Br3C Br1 118.0(8) . . ?
F2 B1 F3 114.0(9) . . ?
F2 B1 F4 112.8(11) . . ?
F3 B1 F4 107.6(9) . . ?
F2 B1 F1 108.9(8) . . ?
F3 B1 F1 106.7(10) . . ?
F4 B1 F1 106.4(8) . . ?
C1S O1S H1S 119.6 . . ?
O1S C1S H1S1 109.5 . . ?
O1S C1S H1S2 109.5 . . ?
H1S1 C1S H1S2 109.5 . . ?
O1S C1S H1S3 109.5 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3B Br2 0.88 2.64 3.351(8) 138.8 . yes
N4 H4B O1W 0.88 2.43 3.11(2) 135.5 . yes
N9 H9A O5W 0.88 2.23 2.938(18) 137.0 . yes
N10 H10B Br3A^a 0.88 2.46 3.215(9) 143.9 . yes
N15 H15A Br3C^c 0.88 2.57 3.439(13) 167.4 . yes
N16 H16B O1S 0.88 2.07 2.85(2) 147.1 . yes
N16 H16B Br1 0.88 2.82 3.407(8) 125.3 . yes
O1S H1S O5W 0.91 2.06 2.88(3) 150.4 . yes

_refine_diff_density_max         1.864
_refine_diff_density_min         -1.668
_refine_diff_density_rms         0.193



